CN110115962A - A kind of synthetic method of silica grafting phenolic resin package reversible color change microcapsule - Google Patents
A kind of synthetic method of silica grafting phenolic resin package reversible color change microcapsule Download PDFInfo
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- CN110115962A CN110115962A CN201910408419.3A CN201910408419A CN110115962A CN 110115962 A CN110115962 A CN 110115962A CN 201910408419 A CN201910408419 A CN 201910408419A CN 110115962 A CN110115962 A CN 110115962A
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- Prior art keywords
- phenolic resin
- silica
- reversible color
- microcapsules
- synthesis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
- C08G8/20—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with polyhydric phenols
- C08G8/22—Resorcinol
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
Abstract
The present invention relates to a kind of synthetic methods of silica grafting phenolic resin package reversible color change microcapsule.The present invention synthesizes synthetic method, and steps are as follows: (1) prepared by mixed emulsifier;(2) synthesis of silica grafting phenolic resin covering material;(3) preparation of the reversible color material shell heart;(4) synthesis of microcapsules.Present invention relates particularly to a kind of synthetic methods of silica grafting phenolic resin package reversible color change microcapsule.Relatively low, the good dispersion of micro capsule technology process energy consumption that the present invention synthesizes, partial size is smaller and cracky, clad ratio be not high.35.5 DEG C of microcapsules discoloring temperature or so, Coloring Time 30s or so, 32 DEG C of secondary color temperature or so, color-recovering time 35s or so, low temperature blue, temperature resistant transparent color, hence it is evident that form microcapsule structure.Regular spherical shape is presented in microcapsules, and partial size is nanoscale.
Description
Technical field
The present invention relates to a kind of synthetic methods of silica grafting phenolic resin package reversible color change microcapsule, specifically relate to
And it is a kind of based on the reversible organic thermo-sensitive material microcapsules of interfacial polymerization synthesis core-shell silica grafting phenolic resin cladding
Synthetic method.
Background technique
Microcapsules refer to a kind of miniature vessel or packing material with polymer wall.Microcapsules granulating technique will exactly be consolidated
Body, liquid or gas entrapment seal the technology for becoming a kind of solia particle product in a kind of microencapsulation up for safekeeping.In recent years, micro-
Capsule technology is widely used in the fixation of microorganism, animal and plant cells, enzyme and other various bioactivators and chemicals
Change aspect.Common micro-capsule is alginic acid/polylysine micro-capsule.Since technology of preparing is more complicated, the saccilar process time is longer,
It has a certain impact, and the price of polylysine is more expensive, thus limits this to the bioactivity for the substance that is embedded
The use of micro-capsule.
The basic material for preparing micro-capsule usually has the polyelectrolyte such as protein, lipid and sugar.Chitosan is that part is sloughed
The chitin of acetyl degree, the latter have excellent toughness and inertia, and hydrophilic, nontoxic, porous, uniform, while chitin is certainly
Content is also very abundant in right boundary.Given this, this test is from the particularity of this natural polymer functional group of chitin, with
And the advantages that nontoxic, hydrophily, sets out, and obtains chitosan with concentrated base is deacetylated, and it is poly- then to reach spherical shell in aforementioned manners
Sugar, and yeast is embedded in globular chitosan with method appropriate, the microcapsules of better performances are prepared, and it is poly- to have inquired into shell
Sugared balling-up condition, the optimum condition for embedding yeast, and feasibility of the chitosan as immobilization material carrier.Traditional micro- glue
Capsule synthetic method is broadly divided into physical method, physico-chemical process, chemical method three classes from principle.Common physical method
There are comminuting method, machine-alloying and an evaporative condenser hair, physical method includes spray drying process, spray chilling method, air suspension, true
Empty evaporation deposition method, complex coacervation, more empty centrifugal process etc.；Physical-chemical process includes aqueous phase separation method, oil-phase separating method, Nang Xinjiao
Change method, extrusion, orifice method, powder bed method；Chemical method includes interfacial polymerization, situ aggregation method, molecule packing method, radiation packet
Capsule method etc..
Nano capsule (nanocapsule) is to be put forward by Narty et al. in late 1970s earliest, is referred generally to
Microcapsules of the partial size between 1-1000nm.Particle size difference is essentially consisted in since Nano capsule is different from common microcapsule,
Therefore when synthesizing Nano capsule, the various factors for influencing partial size should be analyzed to determine technological parameter.Nano capsule
Synthetic method is mainly chemical method and physical-chemical process, wherein Zhu Yinyan et al. is described to synthesize in different colloidal dispersions and be received
The method of rice microcapsules, including interfacial polymerization, interfacial deposition method etc..Recently, it is micro- that nanometer is synthesized using electrodeless metal as wall material
Capsule becomes global hot spot.However the distinct disadvantage of generally production micro capsule technology is complex process, technique synthesis step is more, raw
Production capacity consumes larger and easily broken, water resistance and bad dispersibility, and partial size is universal larger and inhomogenous.
Summary of the invention
The purpose of the present invention is synthesis core-shell silica grafting phenolic resin to coat organic reversible color thermo-sensitive material
The synthetic method of microcapsules, interfacial polymerization can control diameter of particle in the range of smaller and more concentration.Present invention synthesis
Core-shell silica grafting phenolic resin coat the size tunable 50-150nm of organic thermo-sensitive material microcapsules, partial size is smaller
And narrowly distributing, good dispersion, relatively low and non-breakable, the water-tolerant of technical process energy consumption.
A kind of synthetic method of silica grafting phenolic resin package reversible color change microcapsule, the synthetic method are specifically wrapped
It is as follows to include following steps:
(1) mixed emulsifier prepare: under normal temperature condition, take 5g n-hexane and 0.4g Span-80 and 0.1g OP-10 in
100ml beaker stirs 10-20min and obtains solution A after mixing；
(2) under normal temperature condition, 0.1g sodium hydroxide and 3.5g isophthalic the synthesis of silica grafting phenolic resin covering material: are taken
Diphenol is added 100ml distilled water and stirs 10-20min after 200ml beaker, mixing, adds 6ml silica solution reaction 30min, obtains
To solution B；
(3) preparation of the reversible color material shell heart: temperature control is 55 DEG C, and by crystal violet lactone, bisphenol-A, hexadecanol pours into band
Have in the four-hole bottle of blender and dissolve by heating, mixing speed is set as 600-800r/min, and 6g formalin and 0.1g is added
Solution A is slowly dropped in four-hole bottle by OS-10, rate of addition 30-40mL/min, after stirring 30min, obtains emulsion C
And it is cooled to room temperature；
(4) synthesis of microcapsules: under normal temperature condition, solution B being added drop-wise in four-hole bottle, rate of addition 3-4mL/min, stirring
Speed is 600-800r/min, after keeping 5-6h, obtains core-shell silica grafting phenolic resin and coats organic reversible color
Thermo-sensitive material microcapsules.
Synthetic method of the invention has the advantage that
(1) present invention replaces previous thermosetting resin and non-grafted thermoplastic resin using thermoplasticity silica grafting phenolic resin
Rouge synthesizes microcapsules, realizes that partial size is smaller uniform and cracky, clad ratio be not high；
(2) preparation process of microcapsules is essentially room temperature, and operation easy to produce reduces production energy consumption.
Detailed description of the invention
Fig. 1 is the synthetic method that a kind of silica of case study on implementation one is grafted that phenolic resin wraps up reversible color change microcapsule
SEM image.
Fig. 2 is the synthetic method that a kind of silica of case study on implementation two is grafted that phenolic resin wraps up reversible color change microcapsule
SEM image.
Fig. 3 is the synthetic method that a kind of silica of case study on implementation three is grafted that phenolic resin wraps up reversible color change microcapsule
SEM image.
Specific embodiment
The specific embodiment of form by the following examples makees further specifically above content of the invention
It is bright.
Embodiment one:
(1) mixed emulsifier synthesize: under normal temperature condition, take 5g n-hexane and 0.4g Span-80 and 0.1g OP-10 in
100ml beaker stirs 10-20min and obtains solution A after mixing；
(2) under normal temperature condition, 0.1g sodium hydroxide and 3.5g isophthalic the synthesis of silica grafting phenolic resin covering material: are taken
Diphenol is added 80ml distilled water and stirs 10-20min after 200ml beaker, mixing, adds 1ml silica solution reaction 30min, obtains
To solution B；
(3) synthesis of the reversible color material shell heart: temperature control is 55 DEG C, and by crystal violet lactone, bisphenol-A, hexadecanol pours into band
Have in the four-hole bottle of blender and dissolve by heating, mixing speed is set as 600-800r/min, and 6g formalin is added, by solution
A is slowly dropped in four-hole bottle, rate of addition 30-40mL/min, after stirring 30min, is obtained emulsion C and is cooled to room
Temperature；
(4) synthesis of microcapsules: under normal temperature condition, solution B being added drop-wise in four-hole bottle, rate of addition 3-4mL/min, stirring
Speed is 600-800r/min, after keeping 5-6h, obtains core-shell silica grafting phenolic resin and coats organic discoloration temperature-sensitive
Material microcapsule.
35.5 DEG C or so of microcapsules microcapsules discoloring temperature, Coloring Time 30s or so of the implementation case synthesis, secondary color temperature
32 DEG C or so, color-recovering time 35s or so of degree, low temperature blue, temperature resistant transparent color, agglomeration are serious.
Embodiment two:
(1) mixed emulsifier synthesize: under normal temperature condition, take 5g n-hexane and 0.4g Span-80 and 0.1g OP-10 in
100ml beaker stirs 10-20min and obtains solution A after mixing；
(2) under normal temperature condition, 0.1g sodium hydroxide and 3.5g isophthalic the synthesis of silica grafting phenolic resin covering material: are taken
Diphenol is added 80ml distilled water and stirs 10-20min after 100ml beaker, mixing, adds 5ml silica solution reaction 30min, obtains
To solution B；
(3) synthesis of the reversible color material shell heart: temperature control is 55 DEG C, and by crystal violet lactone, bisphenol-A, hexadecanol pours into band
Have in the four-hole bottle of blender and dissolve by heating, mixing speed is set as 600-800r/min, and 6g formalin and 0.1g is added
Solution A is slowly dropped in four-hole bottle by OS-10, rate of addition 30-40mL/min, after stirring 30min, obtains emulsion C
And it is cooled to room temperature；
(4) synthesis of microcapsules: under normal temperature condition, solution B being added drop-wise in four-hole bottle, rate of addition 3-4mL/min, stirring
Speed is 600-800r/min, after keeping 5-6h, obtains core-shell silica grafting phenolic resin and coats organic discoloration temperature-sensitive
Material microcapsule.
35.5 DEG C or so of microcapsules microcapsules discoloring temperature, Coloring Time 30s or so of the implementation case synthesis, secondary color temperature
32 DEG C or so, color-recovering time 35s or so of degree, low temperature blue, temperature resistant transparent color, agglomeration are reduced.
Embodiment three:
(1) mixed emulsifier prepare: under normal temperature condition, take 5g n-hexane and 0.4g Span-80 and 0.1g OP-10 in
100ml beaker stirs 10-20min and obtains solution A after mixing；
(2) under normal temperature condition, 0.1g sodium hydroxide and 3.5g isophthalic the synthesis of silica grafting phenolic resin covering material: are taken
Diphenol is added 80ml distilled water and stirs 10-20min after 200ml beaker, mixing, adds 6ml silica solution reaction 30min, obtains
To solution B；
(3) synthesis of the reversible color material shell heart: temperature control is 55 DEG C, and by crystal violet lactone, bisphenol-A, hexadecanol pours into band
Have in the four-hole bottle of blender and dissolve by heating, mixing speed is set as 600-800r/min, and 6g formalin and 0.1g is added
Solution A is slowly dropped in four-hole bottle by OS-10, rate of addition 30-40mL/min, after stirring 30min, obtains emulsion C
And it is cooled to room temperature；
(4) synthesis of microcapsules: under normal temperature condition, solution B being added drop-wise in four-hole bottle, rate of addition 3-4mL/min, stirring
Speed is 600-800r/min, after keeping 5-6h, obtains core-shell silica grafting phenolic resin and coats organic discoloration temperature-sensitive
Material microcapsule.
35.5 DEG C or so of microcapsules microcapsules discoloring temperature, Coloring Time 30s or so of the implementation case synthesis, secondary color temperature
32 DEG C or so, color-recovering time 35s or so of degree, low temperature blue, temperature resistant transparent color, hence it is evident that form microcapsule structure.
Claims (4)
1. a kind of synthetic method of silica grafting phenolic resin package reversible color change microcapsule, it is characterised in that the method
Steps are as follows:
(1) mixed emulsifier prepare: under normal temperature condition, take 5g n-hexane and 0.4g Span-80 and 0.1g OP-10 in
100ml beaker stirs 10-20min and obtains solution A after mixing；
(2) under normal temperature condition, 0.1g sodium hydroxide and 3.5g the synthesis of silica grafting phenolic resin covering material: are taken
Resorcinol is added 100ml distilled water and stirs 10-20min after 200ml beaker, mixing, adds the reaction of 6ml silica solution
30min obtains solution B；
(3) preparation of the reversible color material shell heart: temperature control is 55 DEG C, and by crystal violet lactone, bisphenol-A, hexadecanol is poured into
Dissolved by heating in four-hole bottle with blender, mixing speed is set as 600-800r/min, and be added 6g formalin and
0.1g OS-10, solution A is slowly dropped in four-hole bottle, rate of addition 30-40mL/min, after stirring 30min,
It obtains emulsion C and is cooled to room temperature；
(4) synthesis of microcapsules: under normal temperature condition, solution B being added drop-wise in four-hole bottle, rate of addition 3-4mL/min, stirring
Speed is 600-800r/min, and after keeping 5-6h, it is organic reversible to obtain core-shell silica grafting phenolic resin cladding
Change colour thermo-sensitive material microcapsules.
2. the synthesis side of a kind of silica grafting phenolic resin package reversible color change microcapsule according to claim 1
Method, it is characterised in that the mass ratio of nonionic surfactant Span-80, OS-10 and OP-10 are 4 in the step (1) (3):
1:1。
3. the synthesis side of a kind of silica grafting phenolic resin package reversible color change microcapsule according to claim 1
Method, it is characterised in that the mass ratio of sodium hydroxide in the step (2), silica solution and resorcinol is 1:70:35.
4. the synthesis side of a kind of silica grafting phenolic resin package reversible color change microcapsule according to claim 1
Method, it is characterised in that crystal violet lactone in the step (3), bisphenol-A, the mass ratio of hexadecanol are 1:3:20.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115895317A (en) * | 2022-11-25 | 2023-04-04 | 山东科技大学 | Hierarchical response self-warning anticorrosive coating and preparation method thereof |
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| JPS58224038A (en) * | 1982-06-24 | 1983-12-26 | Sumitomo Deyurezu Kk | Composition of coated sand and its production |
| CN102827597A (en) * | 2012-06-21 | 2012-12-19 | 天津工业大学 | Thermosensitive discoloring energy-storage material and preparation method thereof |
| US20140338852A1 (en) * | 2011-10-28 | 2014-11-20 | E I Du Pont De Nemours And Company | Treated inorganic pigments having improved dispersability and use thereof in paper products |
| CN105170041A (en) * | 2015-07-13 | 2015-12-23 | 西安理工大学 | Reversible thermochromic microcapsule pigment preparation method |
| CN107224945A (en) * | 2017-06-26 | 2017-10-03 | 西北工业大学 | It is a kind of using phenolic resin be wall material solids as emulsifying agent dicyclopentadiene microcapsule and preparation method |
| CN109173947A (en) * | 2018-09-30 | 2019-01-11 | 江南大学 | A kind of magnetic response electrochromism liquid crystal micro-sphere material and preparation method thereof |
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2019
- 2019-05-16 CN CN201910408419.3A patent/CN110115962A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58224038A (en) * | 1982-06-24 | 1983-12-26 | Sumitomo Deyurezu Kk | Composition of coated sand and its production |
| US20140338852A1 (en) * | 2011-10-28 | 2014-11-20 | E I Du Pont De Nemours And Company | Treated inorganic pigments having improved dispersability and use thereof in paper products |
| CN102827597A (en) * | 2012-06-21 | 2012-12-19 | 天津工业大学 | Thermosensitive discoloring energy-storage material and preparation method thereof |
| CN105170041A (en) * | 2015-07-13 | 2015-12-23 | 西安理工大学 | Reversible thermochromic microcapsule pigment preparation method |
| CN107224945A (en) * | 2017-06-26 | 2017-10-03 | 西北工业大学 | It is a kind of using phenolic resin be wall material solids as emulsifying agent dicyclopentadiene microcapsule and preparation method |
| CN109173947A (en) * | 2018-09-30 | 2019-01-11 | 江南大学 | A kind of magnetic response electrochromism liquid crystal micro-sphere material and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115895317A (en) * | 2022-11-25 | 2023-04-04 | 山东科技大学 | Hierarchical response self-warning anticorrosive coating and preparation method thereof |
| CN115895317B (en) * | 2022-11-25 | 2024-03-12 | 山东科技大学 | Graded response self-early warning anti-corrosion coating and preparation method thereof |
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